安定分子印迹聚合物的制备及应用

Preparation and Application of Diazepam Molecularly Imprinted Polymers

以安定为模板分子,通过本体聚合和沉淀聚合的方法合成了分子印迹聚合物材料,考察了交联剂、致孔剂及温度等条件对聚合物材料性能的影响。电镜扫描图片显示本体聚合得到的聚合物呈不规则形状,而沉淀聚合得到的则是微球颗粒,形状规则。吸附实验表明,聚合物微球对安定的最大吸附量约为130μg/g,对奥沙西泮和硝西泮的吸附量约为110μg/g,对安定类化合物具有较高的吸附性能和选择性。通过对比合成现象和聚合物性能,最终选用以DVB为交联剂、乙腈为致孔剂合成的聚合物微球为固相萃取材料填充固相萃取小柱,从饲料及猪尿样品中选择性地分离、富集痕量安定类药物。结合高效液相色谱法检测,奥沙西泮、硝西泮和安定3种药物在0.1～20 mg/L范围内线性良好,相关系数为0.999 6～0.999 9,检出限(S/N=3)为0.03～0.08 mg/L,加标回收率为66%～79%。该方法为安定类药物的检测提供了一种新途径。

Molecularly imprinted polymer materials were prepared by bulk polymerization and precipitation polymerization methods using diazepam as template molecular,and effects of cross-linker,porogen agent and temperature on the properties of polymer materials were optimized.The molecularly imprinted micropheres were sythesized with divinylbenzene（DVB） as cross-linker and acetonitrile as porogen agent.The polymer prepared by bulk polymerization showed irregular shape,while the micropheres prepared by precipitation polymerization were regular in SEM image.The binding capacity and selective characteristics of the molecularly imprinted polymer were investigated by equilibrium binding experiments.It showed that the maximum adsorption to diazepam of the molecularly imprinted micropheres is up to 130 μg/g and the adsorption to oxazepam and nitrazepam is about 110 μg/g.The results showed that the imprinted polymer exhibited higher adsorptivity and selectivity for diazepam compared with the non-imprinted polymers.In addition,the molecularly imprinted polymer was used as solid phase extraction sorbent in solid-phase extraction column to isolate diazepam in feed and pig urine samples for its excellent identifying characteristics.High performance liquid chromatography（HPLC） was imployed to detect three drugs.The method showed good linearities in the range of 0.1-20 mg/L for oxazepam,nitrazepam and diazepam,with correlation coefficients of 0.999 6-0.999 9 and detection limits（S/N=3） of 0.03-0.08 mg/L.The recoveries of three drug in feed and pig urine were in the range of 71%-79% and 66%-71%,respectively.The proposed method provides a new way for the detection of antipsychotic drugs.